EP4063016A1 - Buse d'atomiseur - Google Patents

Buse d'atomiseur Download PDF

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Publication number
EP4063016A1
EP4063016A1 EP22161529.7A EP22161529A EP4063016A1 EP 4063016 A1 EP4063016 A1 EP 4063016A1 EP 22161529 A EP22161529 A EP 22161529A EP 4063016 A1 EP4063016 A1 EP 4063016A1
Authority
EP
European Patent Office
Prior art keywords
nozzle
bore
tube
atomizer nozzle
base body
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP22161529.7A
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German (de)
English (en)
Inventor
Oliver Beier
Björn MARTIN
Ronny Köcher
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Verein Zur Forderung Von Innovationen Durch Forschung Entwicklung und Technologietransfer Ev (verein Innovent Ev)
Original Assignee
Verein Zur Forderung Von Innovationen Durch Forschung Entwicklung und Technologietransfer Ev (verein Innovent Ev)
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Filing date
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Application filed by Verein Zur Forderung Von Innovationen Durch Forschung Entwicklung und Technologietransfer Ev (verein Innovent Ev) filed Critical Verein Zur Forderung Von Innovationen Durch Forschung Entwicklung und Technologietransfer Ev (verein Innovent Ev)
Publication of EP4063016A1 publication Critical patent/EP4063016A1/fr
Pending legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B7/00—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas
    • B05B7/02—Spray pistols; Apparatus for discharge
    • B05B7/10—Spray pistols; Apparatus for discharge producing a swirling discharge
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B15/00—Details of spraying plant or spraying apparatus not otherwise provided for; Accessories
    • B05B15/60—Arrangements for mounting, supporting or holding spraying apparatus
    • B05B15/65—Mounting arrangements for fluid connection of the spraying apparatus or its outlets to flow conduits
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
    • C23C16/4481—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by evaporation using carrier gas in contact with the source material
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
    • C23C16/4486—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by producing an aerosol and subsequent evaporation of the droplets or particles
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/453—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating passing the reaction gases through burners or torches, e.g. atmospheric pressure CVD
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45563—Gas nozzles
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
    • C23C16/513—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges using plasma jets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B7/00—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas
    • B05B7/02—Spray pistols; Apparatus for discharge
    • B05B7/04—Spray pistols; Apparatus for discharge with arrangements for mixing liquids or other fluent materials before discharge
    • B05B7/0416—Spray pistols; Apparatus for discharge with arrangements for mixing liquids or other fluent materials before discharge with arrangements for mixing one gas and one liquid
    • B05B7/0441—Spray pistols; Apparatus for discharge with arrangements for mixing liquids or other fluent materials before discharge with arrangements for mixing one gas and one liquid with one inner conduit of liquid surrounded by an external conduit of gas upstream the mixing chamber
    • B05B7/045—Spray pistols; Apparatus for discharge with arrangements for mixing liquids or other fluent materials before discharge with arrangements for mixing one gas and one liquid with one inner conduit of liquid surrounded by an external conduit of gas upstream the mixing chamber the gas and liquid flows being parallel just upstream the mixing chamber

Definitions

  • the invention relates to an atomizer nozzle.
  • the invention is based on the object of specifying an improved atomizer nozzle.
  • the tube is guided in the longitudinal direction through the entire atomizer nozzle, in particular its remaining components, including the central bore in the nozzle insert.
  • Leading the tube through the entire atomizer nozzle has the advantage that the media to be atomized are not in contact with the atomizer nozzle or its components, but only with the tube. There is therefore no risk of contamination of the inner nozzle geometry, as the medium is only mixed with the gas at the nozzle outlet. This results in a very long service life for the atomizer nozzle.
  • the tube is formed as a single component throughout its length.
  • a base body is provided with an at least essentially cylindrical receiving bore for receiving the nozzle lance.
  • a gas connection is provided on the base body, which opens into the receiving bore, for example at the side.
  • the base body has a through bore which is arranged coaxially with the receiving bore and serves to receive the tube and/or a guide tube in which the tube is guided.
  • the tube extends longitudinally through the entire atomizer nozzle, including the central bore in the nozzle insert and the guide tube.
  • a first fixing device for the tube is provided on the base body. This allows the tube to be removed and replaced.
  • the tube can be changed, for example, in the event of a blockage. Furthermore, in this way the projection of the tube over the nozzle insert can be varied.
  • a second fixing device is provided for fixing and sealing one end of the nozzle lance in the base body.
  • the second fixing device is designed as a union nut that is screwed onto a thread provided on the base body.
  • the vortex generator is screwed into the free end of the nozzle lance.
  • the nozzle insert is screwed into the vortex generator.
  • the guide tube is guided through the through bore and the central bore of the vortex generator into the cavity within the nozzle insert.
  • the first fixing device is designed as a hollow screw with a central bore, which is screwed or can be screwed into a screw-in hole in the base body, which is arranged coaxially with the through-hole, the screw-in hole having a tapering end in the direction of the through-hole wherein a clamping body is provided at one end of the first fixing device facing the base body, which is pressed together by screwing the first fixing device into the base body in the tapering end of the screw-in hole around the tube and thus fixes it or these.
  • the first fixing device is designed as two hollow screws, each with a central bore.
  • the first banjo bolt is screwed into a screw hole in the base body, with the first banjo bolt having a thread and a shoulder on the inside, on which one or more sealing rings (O-rings, e.g. made of NBR or Viton) can be positioned.
  • the sealing rings around the tube are pressed together via a second hollow screw, which can be screwed into the internal thread of the first hollow screw, and this is thus fixed in the atomizer nozzle.
  • the outer diameter of the tube is in the range from 0.3 mm to 10.0 mm, in particular between 0.6 mm and 3.0 mm.
  • the inner diameter of the tube is in the range from 0.1 mm to 7.0 mm, in particular between 0.1 mm and 2.0 mm.
  • the second fixing device is equipped with magnetic properties and/or with a clamping device in order to hold the atomizer nozzle in a defined, fixed position within a spray chamber or dosing unit.
  • an arrangement for metering a precursor into a gas flow comprising the atomizer nozzle described above and a metering unit, in particular a metering unit according to FIG EP 2 743 373 B1 , wherein the dosing unit comprises a solid base body with a first channel through which a gas flow can flow from a gas inlet to a gas outlet and is introduced as a bore in the base body, wherein a second channel is arranged in the base body, the first channel being under a Angle intersects at a crossing point, with the atomizer nozzle for feeding the precursor into the gas stream being arranged in the second channel, with one end of the second channel being designed as a particle trap below the crossing point when the dosing unit is in a position of use, with a cleaning opening that can be closed with a sealing plug for the particle trap is provided.
  • the atomizing nozzle can be used for atomizing various media, such as a liquid, a liquid mixture, a solution, a dispersion, a suspension or an emulsion, which is carried in the tube.
  • the medium is atomized in a gas stream emerging from the central bore of the nozzle insert, the atomized medium being used in a process for chemical and/or physical vapor deposition, for spray pyrolysis, for the spray application of paints, primers, sol-gel mixtures, adhesives , for electrospinning, for suspension plasma spraying, for spray drying (atomization drying) to produce fine powders or generally for aerosol production, e.g ) is used.
  • the nozzle system newly developed here is one of the two-substance nozzles with external mixing.
  • Such a type of nozzle is particularly suitable for coating processes and here in particular for chemical vapor deposition (CVD) and its special cases PECVD, APPCVD, CCVD.
  • CVD chemical vapor deposition
  • atomizers are among the preferred methods for preparing precursors in the field of CVD and thin-film technology in general (e.g. sol-gel applications).
  • the invention relates to an atomizer nozzle and a method for converting a medium, for example a liquid, a liquid mixture, a solution, a dispersion, suspension or emulsion, in particular a liquid precursor, into fine droplets (aerosol form) for use in coating processes.
  • a medium for example a liquid, a liquid mixture, a solution, a dispersion, suspension or emulsion, in particular a liquid precursor
  • APPCVD plasma-enhanced chemical vapor deposition at atmospheric pressure
  • CCVD combustion CVD, also known as flame coating
  • the atomizer nozzle and/or the process are not limited to these two processes, but can also be used for spray pyrolysis or for spray application of paints, primers, sol-gel mixtures, adhesives or liquid chemicals in general (pure substances, mixtures of substances, solutions, dispersions , suspensions, emulsions), low-pressure plasma deposition (PECVD), atmospheric sputtering techniques, suspension plasma spraying or as a nozzle for electrospinning.
  • PECVD low-pressure plasma deposition
  • the atomizer nozzle enables homogeneous aerosol generation over a wide range of flow rates, from around 0.1 ⁇ l/min up to 2000 ml/min depending on the inner diameter of the tube selected.
  • the nozzle principle is therefore suitable for small individual systems, for example atmospheric plasma jets, up to scaled-up plasma or flame treatment systems (system widths from several centimeters to meters). to supply precursors.
  • All types of displacement pumps can be used as pump types for conveying the medium in the direction of the atomizer nozzle, with hose pumps (peristaltic pumps) preferably being used.
  • the atomizer nozzle can also be operated without a pump, using the Venturi effect. In this case, the atomizer nozzle has self-priming properties for the medium (self-priming two-substance nozzle).
  • figure 1 is a schematic view of the atomizing nozzle D.
  • figure 2 is another schematic view of the atomizing nozzle D.
  • the atomizer nozzle D comprises a first fixing device 1 for a tube 9, for example a pump hose 9 or a cannula 9, a guide tube 2, a gas connection 3, a base body 4, a second fixing device 5 for a nozzle lance 6, a vortex generator 7, a nozzle insert 8 and a tube 9, for example a pump tube 9 or a cannula 9.
  • a spray cone 10 emerging from the atomizer nozzle D is also shown.
  • the base body 4 has an at least essentially cylindrical receiving bore 4.1 for receiving the nozzle lance 6.
  • the gas connection 3 is provided, for example, on the side of the base body 4 and opens into the receiving bore 4.1.
  • the base body 4 also has a through hole 4.2, which can be arranged coaxially with the receiving hole 4.1, but can have a smaller diameter than this.
  • the through hole 4.2 serves to accommodate the guide tube 2.
  • the second fixing device 5 serves to fix one end of the nozzle lance 6 in the base body 4 and is designed, for example, as a union nut that can be screwed onto an external thread provided on the base body 4.
  • At least one seal can be provided in the second fixing device 5 , which seals against the nozzle lance 6 when the second fixing device 5 is screwed on and clamps it in the second fixing device 5 .
  • the nozzle lance 6 can be equipped with an external thread on one side and the base body 4 with an internal thread in order to screw the nozzle lance 6 into the base body 4 .
  • the vortex generator 7 is arranged, for example screwed.
  • the nozzle insert 8 is arranged downstream of the vortex generator 7 , for example screwed into the vortex generator 7 .
  • the vortex generator 7 and the nozzle insert 8 each have a central bore 7.1, 8.1, which are arranged coaxially with the through bore 4.2 when the nozzle lance 6 is arranged in the base body 4, the vortex generator 7 in the nozzle lance 6 and the nozzle insert 8 in the vortex generator 7 or in the nozzle lance 6 is.
  • the guide tube 2 is guided through the through bore 4.2 and the central bore 7.1 of the vortex generator 7 into a cavity 8.2 within the nozzle insert 8.
  • the guide tube 2 can be fixed in the through hole 4.2 and/or in the central hole 7.1 in the vortex generator 7, for example by being pressed in.
  • the tube 9 is guided in the longitudinal direction through the entire atomizer nozzle D, ie through the guide tube 2 and the central bore 8.1 in the nozzle insert 8, and is fixed by the first fixing device 1 by pressing on it.
  • the first fixing device 1 can be designed as a hollow screw with a central bore which is screwed or can be screwed into a screw-in bore 4.3 which is arranged coaxially with the through-hole 4.2.
  • the screw-in hole 4.3 has a tapering end in the direction of the through-hole 4.2.
  • a clamping body 1.1 is provided which, when the first fixing device 1 is screwed into the base body 4, is pressed together in the tapering end of the screw-in hole 4.3 around the tube 9 and thus fixes it .
  • the first fixing device 1 can be designed as two hollow screws, each with a central bore.
  • the first banjo bolt 1.2 is screwed into a screw-in hole 4.3 in the base body 4, with the first banjo bolt 1.2 having a thread and a shoulder on the inside, on which one or more sealing rings (O-rings, e.g. made of NBR or Viton) can be positioned.
  • the sealing rings are pressed together around the tube 9 and this is thus fixed in the atomizer nozzle D via a second hollow screw 1.3, which can be screwed into the internal thread of the first hollow screw 1.2.
  • the inner diameter of the central bores 7.1, 8.1 of the first fixing device 1, the vortex generator 7 and the nozzle insert 8 as well as the Guide tube 2 are matched on the one hand to each other and on the other hand to the maximum outer diameter of the tube 9 .
  • Other tube geometries can be used by structural adjustments, in particular changing the inner diameter, of these four parts.
  • the outer diameter of the tube 9 is, for example, in the range from 0.3 mm to 10.0 mm, particularly preferably between 0.6 mm and 3.0 mm.
  • the inner diameters are, for example, correspondingly in the range from 0.1 mm to 7.0 mm, particularly preferably between 0.1 mm and 2.0 mm.
  • the gas connection 3 enables the gas supply to the atomizer nozzle D, with all gases and gas mixtures being able to be used.
  • the gas connection 3 and thus the atomizer nozzle D can particularly preferably be operated with compressed air, synthetic air, nitrogen, argon, helium or nitrogen-hydrogen gas mixtures (forming gas).
  • the atomizer nozzle D can be integrated into spray chambers or dosing units via the second fixing device 5 or the nozzle lance 6 .
  • the dosing unit can, for example, as in EP 2 743 373 B1 be formed, the entire contents of which are hereby incorporated by reference.
  • the second fixing device 5 can be equipped with magnetic properties, for example, so that the atomizer nozzle D can be held in a defined, fixed position within a spray chamber or dosing unit.
  • the second fixing device 5 has a permanent magnetic material or a magnetizable material that is or can be held by a permanent magnet arranged on the spray chamber or dosing unit.
  • a structural mount can be provided on the nozzle lance 6 (e.g. via sealing rings, whereby gas/liquid tightness at the transition to the spray chamber is possible at the same time) or the atomizer nozzle D can be connected via a clamping device (e.g a bayonet catch, a hinge, a thread, a compression fitting or a union nut) can be fixed to the spray chamber or dosing unit.
  • a clamping device e.g a bayonet catch, a hinge, a thread, a compression fitting or a union nut
  • the vortex generator 7 is used for the targeted turbulence of the gas introduced via the gas connection 3 , which flows through the receiving bore 4 . 1 and the nozzle lance 6 to the vortex generator 7 .
  • the vortex generator 7 has at least one channel 7.2, which is spaced radially from the central bore 7.1.
  • two, three, four, five or more channels 7.2 can be provided, which can be arranged uniformly around the central bore 7.1.
  • the channel 7.2 can be designed, for example, as an oblique bore, ie not parallel to the central bore 7.1, or as a section of a helix.
  • the gas thus gets swirled into the cavity 8.2 of the nozzle insert 8 and through its central bore 8.1.
  • the nozzle insert 8 can preferably be designed as a full cone nozzle (spray pattern corresponds to a circular area), but can also be designed as a hollow cone nozzle or flat jet nozzle.
  • the resulting spray angle can be determined via the relative positioning of the tube 9 to the nozzle insert 8 in the longitudinal direction, via the diameter of the central bore 8.1 of the nozzle insert 8 and the tube 9, via a variation in the pressure of the gas and/or the gas flow and/or the amount of the Medium and / or on the type of medium (for example, its viscosity) can be adjusted.
  • the spray angles are, for example, between 5° and 120°, particularly preferably between 10° and 60°.
  • the gas flow can be between 1 l/min and 100 l/min, particularly preferably between 2 l/min and 30 l/min.
  • the components of the atomizer nozzle D can consist of any suitable material, for example steel, stainless steel, brass, aluminium, plastics such as POM or PTFE or glass/ceramics.
  • the aerosols generated by the atomizer nozzle D were analyzed by means of scattered light measurements.
  • a HELOS KR-H2487 laser diffraction spectrometer (laser wavelength: 632.8 nm) was used for this purpose, and the aerosols were sprayed into the analysis area.
  • the Fraunhofer theory was used to evaluate the measurement signal.
  • the atomizer nozzle D was operated with a cannula 9 made of stainless steel with an external diameter of 0.8 mm. Compressed air was used as the gas. The gas pressure at the atomizer nozzle D was varied from 1 bar to 6 bar.
  • test media used were two precursor liquids for APPCVD and CCVD coating processes, tetraethoxysilane (TEOS) for the production of silicon oxide layers and dissolved zinc nitrate (solvent: H 2 O / isopropanol with a volume ratio of 1:1) for zinc oxide layers or composite layers embedded in the zinc oxide particles (e.g. for layers with antimicrobial properties).
  • TEOS tetraethoxysilane
  • solvent H 2 O / isopropanol with a volume ratio of 1:1
  • the two solvents used were distilled H 2 O and a H 2 O / isopropanol mixture with a volume ratio of 1:1.
  • the media were metered into the atomizer nozzle D using a peristaltic pump and a constant flow rate of 100 ⁇ l/min.
  • volume-weighted droplet distributions of the four types of aerosol for pressures at the atomizer nozzle D of 1 bar to 6 bar are shown.
  • the volume-weighted droplet size distribution of the primary precursor aerosols at the atomizer nozzle D is shown for the precursors TEOS (top left), zinc nitrate (top right) and the solvents H 2 O (bottom left), H 2 O / isopropanol mixture by volume 1:1 (bottom right).
  • the geometric equivalent diameter x geo is plotted on the abscissa in the unit ⁇ m.
  • the atomizer nozzle D has a bimodal droplet size distribution. That is, there are two intensity maxima. With increasing nozzle pressure, the droplet distributions are shifted to smaller particle sizes for all test media. Furthermore, the concentrations of droplets + ⁇ 1 ⁇ m increase significantly, which are of particular interest for coating processes.
  • the atomizer nozzle D is used in this example with a spray chamber according to EP 2 743 373 B1 combined.
  • the structure and selected parameters of the atomizer nozzle D are identical to example 1.
  • TEOS and dissolved zinc nitrate represent the two test media.
  • the droplet size distribution was analyzed using a laser diffraction spectrometer this time at the outlet of the spray chamber (with integrated atomizer nozzle D).
  • figure 4 are the volume-weighted droplet distributions for pressures at the atomizer nozzle D from 1 bar to 6 bar at the outlet of the spray chamber according to EP 2 743 373 B1 shown for the precursors TEOS (left) and zinc nitrate (right).
  • the combination of spray chamber and atomizer nozzle D achieves a monomodal distribution and a limitation of the maximum droplet sizes for both precursor types, especially at high pressures. Furthermore, there is a shift in the mean droplet sizes to lower values (approx. 1 ⁇ m in the case of volume-weighted representation). In these investigations, too, an increase in pressure from 1 bar to 6 bar leads to an increase in the concentration of droplets ⁇ 1 ⁇ m.
  • a pump tube 9 made of PTFE (polytetrafluoroethylene) was fixed inside the atomizer nozzle D with the aid of the first fixing device 1 .
  • the outside diameter of the pump hose 9 is 0.8 mm, the inside diameter 0.3mm Ethanol served as the test liquid, which was metered into a carrier gas (compressed air at 15 l/min) via the atomizer nozzle D and passed on to a gas measuring cell.
  • the ethanol concentration inside the gas measuring cell is analyzed with a gas sensor of the type Dräger Pac 8000 OV-A (measuring range: 0 - 300 ppm) under constant flow.
  • the ethanol flow rate at the atomizer nozzle D was varied between 2.0 ⁇ l/min and 9.0 ⁇ l/min using a peristaltic pump.
  • FIG 5 shows the ethanol concentration in the gas measuring cell as a function of the ethanol flow rate at the atomizer nozzle D (between 2.0 ⁇ l/min and 9.0 ⁇ l/min). Each dosing rate was measured for five minutes and the ethanol concentration was documented every 30 seconds. The measured values shown are averaged over seven individual measurement series.
  • the result shows a linear increase in the ethanol concentration in the gas measuring cell with the ethanol flow rate.
  • the high process stability is also figure 6 shows where the gas concentration for ethanol flow rates of 2 ⁇ l/min and 7 ⁇ l/min was measured at nebulizer nozzle D over a measurement time of 50 minutes.
  • figure 6 shows a diagram of the gas concentration as a function of the measurement time within a gas measurement cell for ethanol flow rates of 2 ⁇ l/min and 7 ⁇ l/min at atomizer nozzle D.
  • the coefficient of variation was 4.5% for 2 ⁇ l/min and 0.5% for 7 ⁇ l/min. It should be noted here that the measurement accuracy of the gas sensor is specified as ⁇ 20% of the measured value and the error at low gas concentrations may be at the upper end of the error tolerance.
  • a commercial MEF plasma jet (Tigres GmbH) was used for the plasma tests (APPCVD).
  • An HMDSO/isopropanol mixture served as a precursor.
  • the atomizing nozzle D is provided with a spray chamber according to EP 2 743 373 B1 combined and the atomized precursor conducted from the outlet of the spray chamber to the plasma.
  • the atomizer nozzle D was operated with a cannula 9 made of stainless steel with an external diameter of 0.8 mm, the precursor flow rate was 40 ⁇ l/min and the gas pressure was 4 bar. Compressed air was used as the gas.
  • the coating was carried out with constant plasma parameters on previously masked glass slides and silicon wafers as follows:
  • the atomizer nozzle D was operated continuously over a period of eight hours in order to assess the long-term dosing stability. After one hour in each case, the SiOx coating of the substrates took place with the parameters mentioned above. Finally, the layer thickness (difference in height: layer/substrate) was evaluated using an Alpha-Step D-600 profilometer from KLA Tencor after removal of the masking. In figure 7 the results are shown. figure 7 shows a diagram for displaying layer thicknesses in Dependence on a coating time to assess the long-term dosing stability of the atomizer nozzle D.
  • the layer thicknesses on the glass substrates were approximately 130 nm to 145 nm and 105 nm to 115 nm on the Si wafers. Without taking into account the fluctuations in the plasma process, the coefficient of variation was less than 5% over the eight-hour dosing time.
  • the coating was carried out with the following parameters of the flame system on previously masked float glass (100 mm x 50 mm x 4 mm) on the glass air side:
  • the layer thickness was measured using a KLA Tencor Alpha-Step D-600 profilometer. A very high level of uniformity was found across the coated glass width, the average layer thickness was in the range of approx. 50 nm.

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EP22161529.7A 2021-03-25 2022-03-11 Buse d'atomiseur Pending EP4063016A1 (fr)

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Publication number Priority date Publication date Assignee Title
US3586240A (en) * 1968-11-29 1971-06-22 Nippon Kokan Kk Blowing nozzle
EP0000002B1 (fr) 1977-06-01 1981-08-26 Bayer Ag Dérivés du tétrahydrofuranne, leurs procédés de préparation et leur utilisation comme herbicides
DE19509223C1 (de) * 1995-03-17 1996-11-07 Holger Schrader Mehrstoff-Zerstäuberdüse
US20030136861A1 (en) * 2002-01-24 2003-07-24 Kangas Martti Y.O. Low pressure atomizer for difficult to disperse solutions
DE102007055936A1 (de) * 2007-12-30 2009-07-09 Georg-August-Universität Göttingen Stiftung Öffentlichen Rechts Aerosolerzeugerdüse, Aerosolerzeugersystem, Beschichtungssystem und Verfahren
US20110192909A1 (en) * 2010-02-05 2011-08-11 Msp Corporation Fine droplet atomizer for liquid precursor vaporization
DE102012220986A1 (de) * 2012-11-16 2014-05-22 Innovent E.V. Technologieentwicklung Dosiereinheit und Verfahren zur Abscheidung einer Schicht auf einem Substrat

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Publication number Priority date Publication date Assignee Title
CA988557A (en) 1972-09-18 1976-05-04 Albert H. Moos Apparatus for and method of spraying plural component materials
US6699365B2 (en) 2001-10-22 2004-03-02 Abb Inc. Method of wetting webs of paper or other hygroscopic material
AU2003291973A1 (en) 2002-12-20 2004-07-14 Lifecycle Pharma A/S A self-cleaning spray nozzle
DE102017120468B3 (de) 2017-09-06 2018-05-09 I.T.C. Intercircuit Production GmbH Lack-Beschichtungseinrichtung

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3586240A (en) * 1968-11-29 1971-06-22 Nippon Kokan Kk Blowing nozzle
EP0000002B1 (fr) 1977-06-01 1981-08-26 Bayer Ag Dérivés du tétrahydrofuranne, leurs procédés de préparation et leur utilisation comme herbicides
DE19509223C1 (de) * 1995-03-17 1996-11-07 Holger Schrader Mehrstoff-Zerstäuberdüse
US20030136861A1 (en) * 2002-01-24 2003-07-24 Kangas Martti Y.O. Low pressure atomizer for difficult to disperse solutions
DE102007055936A1 (de) * 2007-12-30 2009-07-09 Georg-August-Universität Göttingen Stiftung Öffentlichen Rechts Aerosolerzeugerdüse, Aerosolerzeugersystem, Beschichtungssystem und Verfahren
US20110192909A1 (en) * 2010-02-05 2011-08-11 Msp Corporation Fine droplet atomizer for liquid precursor vaporization
DE102012220986A1 (de) * 2012-11-16 2014-05-22 Innovent E.V. Technologieentwicklung Dosiereinheit und Verfahren zur Abscheidung einer Schicht auf einem Substrat
EP2743373B1 (fr) 2012-11-16 2015-06-24 Innovent e.V. Unité de dosage et son utilisation

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
G. WOZNIAK: "Zerstäubungstechnik - Prinzipien, Verfahren", 2003, SPRINGER-VERLAG

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